Redetermination of tris(N,N-diethyldithiocarbamato)antimony(III)

Abstract

The title compound, [Sb(C5H10NS2)3], was synthesized from Sb2O3, diethyl­amine, carbon dis­ulfide, hydro­chloric acid and sodium hydroxide. The structure has been published previously but H atoms were not included in the model [Raston & White (1976 ▶). Chem. Soc. Dalton Trans. p. 791]. The current determination has significantly higher precision than the original work. The complex has three ligands. The Sb atom is coordinated by three bidentate diethyl­dithio­carbamate groups, two in an almost planar fashion and the third perpendicular to that plane with a dihedral angle of 86.429 (13)°. One ethyl group is disordered over two positions of equal occupancy.

Resolvable polymorphism in an intergrowth of two modifications of tris(diethyldithiocarbamato)antimony

“…2) forms. The triclinic polymorph is a new polymorph, whereas the monoclinic polymorph has been reported previously (Raston & White, 1976;Que et al, 2009). The triclinic polymorph is marginally denser.…”

“…Polymorphism has been the subject of several reviews (Braga et al, 2009;Brog et al, 2013;Kersten et al, 2018;Purohit & Venugopalan, 2009; Sá nchez-Fé rez & Pons, 2021), but these do not furnish refer-ences on stereochemically-active metal complexes. The specimen should be a single-phase crystal consisting of two intergrown polymorphs, but unfortunately the synthesis was not reproducible, and several atttempts gave only the monoclinic modification, which has already been reported (Raston & White, 1976;Que et al, 2009). The diffraction images did not show any streaking; the well-separated spots constrasted with the streaks in the images observed for the class of ordereddisordered structures (Hans et al, 2015;Strand et al, 2016).…”

“…The compound was synthesized by the reaction of antimony chloride and sodium diethyldithiocarbamate according to the procedure reported for monoclinic tris(diethyldithiocarbamato)antimony (Raston & White, 1976;Que et al, 2009). Large orange crystals were obtained upon recrystallization from ethanol that were shown to be the presumed allotwin.…”

Supramolecular associationviaSb...S and C—H...S interactions in dimerictris(N,N-dimethyldithiocarbamato-S,S′)antimony(III): an approach to overcome the concept of steric bulk on such interactions

“…We have compared the supramolecular interactions of the title compound with the previously reported Sb(S 2 CNR 2 ) 3 analogues, R = alkyl and/or aryl, to ascertain the novelty of the compound. The diethyl analogue has been determined twice (Raston & White, 1976;Que et al, 2009) and exhibits noncrystallographic C s symmetry. Interestingly, similar geometry is found but merely strong [3.389 (4) Å ] SbÁ Á ÁS interactions exist between symmetry-related molecules.…”